Water → 3-(4-Chloromethyl-2-methyl-phenyl)-propionic Acid Methyl Ester
反応式
[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12]O)=[CH:8][C:7]=1[CH3:14].C(N(CC)CC)C.S(Cl)([Cl:25])=O.O>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][Cl:25])=[CH:8][C:7]=1[CH3:14]参加物
6
実験手順
To a 0° C. solution of 3-(4-Hydroxymethyl-2-methyl-phenyl)-propionic acid methyl ester (1.02 g, 4.90 mmol) in anhydrous CH2Cl2 (15 mL) is added triethylamine (0.75 mL, 5.38 mmol) followed by thionyl chloride (0.40 mL, 5.48 mmol). The mixture is allowed to warm to RT overnight. Water is added, and the mixture is extracted with CH2Cl2. The organics are dried with MgSO4 and concentrated. The crude material is purified by flash chromatography to yield the title compound (1.01 g, 91%).
後処理
- extractionthe mixture is extracted with CH2Cl2
- dry with materialThe organics are dried with MgSO4
- concentrationconcentrated
- customThe crude material is purified by flash chromatography
出典と根拠
- ORDレコード
- ord-061c43d2dd0e427a9fd96a6b2d184653
- 出典データセット
- uspto-grants-2006_12
- 特許番号
- US07153878B2
反応ノート
読み込み中…